反应方程式
C1CCNC1.O=Cc1cc(F)ccc1Br>CC(=O)O.CC(=O)O.Cc1ccccc1.O=C([O-])[O-].[Cs+].[Cs+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>O=Cc1cc(F)ccc1N1CCCC1参与物
7
反应条件
- 温度
- 95 °C
实验过程
To a mixture of pyrrolidine (328 mg, 3.05 mmol), 2-bromo-4-fluorobenzaldehyde (619 mg, 3.05 mmol) in toluene (10 ml) was added Cs2CO3 (2.48g, 7.62 mmol), BINAP (95 mg ) and palladium(II) acetate (35 mg) was added. The mixture was purged with Ar for 5 min, then heated at 95 oC for 4 hrs. After cooled to RT, EtOAc (30 mL) was added. The organic layer was washed with water (3 x 30 mL), brine (30 mL), dried over MgSO4, filetred and concentrated. The residue was purified via combiflush (0 - 20% EtOAc/Hexane; 40 g column) to give the desired product as a clear reddish liquid. LCMS and H-NMR look good. 290 mg Conclusion: reaction progressed to give desired product in 49% yield.
来源与证据
- ORD记录
- ord-ac71d193208d45949ee247d7a0855249
- 来源数据集
- 750 AstraZeneca ELN dataset
- 原始链接
- 查看来源
关联笔记
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